CN106011852B - A kind of preparation method of austenite stainless steel surface high entropy alloy coating - Google Patents

A kind of preparation method of austenite stainless steel surface high entropy alloy coating Download PDF

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CN106011852B
CN106011852B CN201610382380.9A CN201610382380A CN106011852B CN 106011852 B CN106011852 B CN 106011852B CN 201610382380 A CN201610382380 A CN 201610382380A CN 106011852 B CN106011852 B CN 106011852B
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stainless steel
entropy alloy
workpiece
alloy coating
high entropy
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CN106011852A (en
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林乃明
杨慧君
邹娇娟
王思
乔珺威
王振霞
马永
唐宾
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Shandong Huada Jinke New Material Co ltd
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Taiyuan University of Technology
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    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C26/00Coating not provided for in groups C23C2/00 - C23C24/00
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25FPROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
    • C25F3/00Electrolytic etching or polishing
    • C25F3/02Etching
    • C25F3/06Etching of iron or steel

Abstract

The invention discloses a kind of preparation methods of austenite stainless steel surface high entropy alloy coating, belong to technical field of metal material surface modification.Include the following steps: for austenitic stainless steel test piece to be placed in sodium chloride solution, processing is performed etching to it using Electrochemical Measurement Technology, the austenite stainless steel workpiece that electrochemical etching is handled well is connect with the cathode of metal surface enhanced processor power supply, as workpiece pole, comb shape high entropy alloy material is connect by fixture with the anode of metal surface enhanced processor power supply again, becomes machined electrode;Power on, apply DC voltage between workpiece pole and machined electrode, in austenite stainless steel workpiece surface with 0.5~1.5 cm2/ min rate moves machined electrode, cuts off the power after processing is completed, workpiece is made to be cooled to room temperature.The large area of austenite stainless steel surface high entropy alloy coating, quickly preparation can be achieved in the present invention, and high entropy alloy coating obtained has good wearability.

Description

A kind of preparation method of austenite stainless steel surface high entropy alloy coating
Technical field
The present invention relates to a kind of preparation methods of austenite stainless steel surface high entropy alloy coating, belong to metal material surface Technical field of modification.
Background technique
Austenitic stainless steel is because having good comprehensive mechanical property and processing performance, and in oxidisability and reductant In show preferable corrosion resistance, to be widely used in the fields such as industrial, civilian, national defence.Currently, Ovshinsky Body stainless steel is also most species in stainless steel, a kind of maximum steel of usage amount, and output and usage amount account for about stainless steel More than half of total output and usage amount.But, coefficient of friction low by surface hardness is big, the disadvantages of wearing no resistance is restricted, It is more widely used and is restricted, austenitic stainless steel fundamentally cannot be used production sliding friction and match secondary components.Based on friction Abrasion, which originates, is born in material surface, and existing research shows the wearability that austenitic stainless steel can be effectively improved by sufacing. Select suitable process for treating surface that there is significant meaning for expanding austenitic stainless steel as the application of friction material.
High-entropy alloy possesses high rigidity, high intensity, good wearability, corrosion resistance, resistance to high temperature oxidation and high temperature creep-resisting Etc. excellent performance, in the fields such as aerospace, electronics, machine-building and metallurgy, chemical industry, the energy as high-strength, wear-resisting, resistance to High temperature, corrosion resistant material etc. are with a wide range of applications.High-entropy alloy earns widespread respect as the application prospect of wear-resistant material, But current high-entropy alloy mainly uses vacuum arc melting and casting method to prepare, and needs to have coloured gold using more valuableness Belong to, it is very high to be manufactured directly to block materials cost.High entropy alloy coating is formed using sufacing, can play and utilize high entropy The advantage of alloy effectively overcomes the problems, such as cost and processing, and significantly improves the wearability of respective substrates material.
Summary of the invention
The present invention is intended to provide a kind of preparation method of austenite stainless steel surface high entropy alloy coating, resulting high entropy is closed Gold plating is remarkably improved the wearability of austenitic stainless steel, reduces wear weight loss.
The present invention provides a kind of preparation methods of austenite stainless steel surface high entropy alloy coating, first not to austenite The steel that becomes rusty carries out electrochemical etching processing, then prepares high entropy alloy coating again.
Above-mentioned preparation method, specifically includes the following steps:
(1) austenite stainless steel workpiece is pre-processed: silicon carbide water will be used after austenitic stainless steel strip oil removing Sand paper is polished step by step, distilled water is cleaned by ultrasonic, drying for standby;
(2) the austenitic stainless steel test piece pre-processed is reserved into working face, rest part is sealed using epoxy resin, is dry After dry, as working electrode, it is molten to be placed in the sodium chloride that mass percent is the % of 10 % ~ 25 with reference electrode and auxiliary electrode In liquid, three-electrode system is formed, electrochemical etching processing is carried out to austenitic stainless steel test piece using electrochemical workstation, is obtained Austenite stainless steel workpiece;
(3) cathode of the austenite stainless steel workpiece for handling step (2) well and metal surface enhanced processor power supply connects It connects, becomes workpiece pole, then connect comb shape high-entropy alloy with the anode of metal surface enhanced processor power supply by fixture, at For machined electrode;
(4) power supply for connecting metal surface enhanced processor, applies the straight of 80 ~ 100 V between workpiece pole and machined electrode Galvanic electricity pressure, the air quilt when the distance between workpiece pole and machined electrode are lower than 0.1 mm, between workpiece pole and machined electrode Ionization generates gas discharge phenomenon, that is, starts the preparation that high entropy alloy coating is carried out to austenite stainless steel workpiece;
(5) to austenite stainless steel workpiece surface continue through-current capacity be 6000~8000 sccm argon gas, austenite not The mobile machined electrode of the steel workpiece surface that becomes rusty, makes electro-discharge machining rate control in 0.5~1.5 cm2/ min, process time be 1.5~ 3 h cut off the power supply of metal surface enhanced processor after processing is completed, are further continued for logical 5~15 min of argon gas, make austenite stainless Steel workpiece is cooled to room temperature.
In above-mentioned preparation method, the austenitic stainless steel is 316L austenitic stainless steel.
In above-mentioned preparation method, the high-entropy alloy is AlCrCuFeNi2Multicomponent high-entropy alloy.
In above-mentioned preparation method, the mass percent of the sodium chloride solution is 15 % or 20 %.
In above-mentioned preparation method, the reference electrode is saturated calomel electrode;The auxiliary electrode is platinized platinum.
In above-mentioned preparation method, in step (5), the DC voltage is 80 V or 90 V, and processing speed is 1 cm2/ Min, process time are 2 h.
High-entropy alloy used in the present invention is comb shape, is needed because high-entropy alloy is more demanding to preparation condition Quickly solidification, the scantling that can be prepared is all little, so small ear of maize or flakelet can only be made at present, it is referred to herein Comb shape high-entropy alloy refer to multiple high-entropy alloy spillikin subgroups altogether, look at as comb.
Beneficial effects of the present invention:
The invention belongs to technical field of metal material surface modification, using austenitic stainless steel to Cl-Pitting Susceptibility is high The characteristics of, electrochemical etching processing first is carried out to 316L stainless steel and obtains Surface Texture, then prepares high entropy alloy coating.The present invention The advantages of be can austenite stainless steel surface realize high entropy alloy coating large area, quickly preparation, good effect is institute The high entropy alloy coating of acquisition has good wearability, reduces wear weight loss.
Detailed description of the invention
Fig. 1 is the X-ray diffractogram of high-entropy alloy and high entropy alloy coating;The X-ray diffraction of 1-high-entropy alloy in figure Spectrum;The X-ray diffraction spectrum of 2-high entropy alloy coatings;
Fig. 2 is the abrasion of untreated austenitic stainless steel and embodiment 1 treated austenitic stainless steel and GCr15 opposite grinding Weightlessness figure;The wear weight loss figure of 3-untreated austenitic stainless steels and GCr15 opposite grinding in figure;4-embodiment, 1 high-entropy alloy applies The wear weight loss figure of layer and GCr15 opposite grinding;
Fig. 3 is untreated austenitic stainless steel and embodiment 1 treated austenitic stainless steel and Si3N4The abrasion of opposite grinding Weightlessness figure;5-untreated austenitic stainless steels and Si in figure3N4The wear weight loss figure of opposite grinding;6-embodiment, 1 high entropy alloy coating With Si3N4The wear weight loss figure of opposite grinding;
Fig. 4 is the abrasion of untreated austenitic stainless steel and embodiment 2 treated austenitic stainless steel and GCr15 opposite grinding Weightlessness figure;The wear weight loss figure of 7-untreated austenitic stainless steels and GCr15 opposite grinding in figure;8-embodiment, 2 high-entropy alloy applies The wear weight loss figure of layer and GCr15 opposite grinding;
Fig. 5 is untreated austenitic stainless steel and embodiment 2 treated austenitic stainless steel and Si3N4The abrasion of opposite grinding Weightlessness figure;9-untreated austenitic stainless steels and Si in figure3N4The wear weight loss figure of opposite grinding;10-embodiment, 2 high-entropy alloy applies Layer and Si3N4The wear weight loss figure of opposite grinding.
Specific embodiment
The present invention is further illustrated below by embodiment, but is not limited to following embodiment.
Embodiment 1:
Now by taking 316L austenitic stainless steel as an example, the present invention is implemented:
Embodiment 1:
(1) austenite stainless steel workpiece is pre-processed: silicon carbide water will be used after austenitic stainless steel strip oil removing Sand paper is polished step by step, distilled water is cleaned by ultrasonic, drying for standby;
(2) the austenitic stainless steel test piece pre-processed is reserved into working face, rest part is sealed using epoxy resin, is dry It is dry after, as working electrode, with the saturated calomel electrode as reference electrode and as the large area platinized platinum of auxiliary electrode Be placed in mass percent be 20 % sodium chloride solution in, form three-electrode system, by electrochemical workstation to austenite not Steel test piece of becoming rusty carries out electrochemical etching processing, obtains austenite stainless steel workpiece;
(3) cathode of the austenite stainless steel workpiece for handling step (2) well and metal surface enhanced processor power supply connects It connects, becomes workpiece pole, then connect comb shape high-entropy alloy with the anode of metal surface enhanced processor power supply by fixture, at For machined electrode;
(4) power supply of metal surface enhanced processor is connected, selection applies DC voltage between workpiece pole and machined electrode 80 V, when the distance between workpiece pole and machined electrode are lower than 0.1 mm, the air between workpiece pole and machined electrode is electric From generation gas discharge phenomenon can start the preparation for carrying out high entropy alloy coating to austenite stainless steel workpiece;
(5) keeping the DC voltage between workpiece pole and machined electrode is 80 V, starts prepares coating: to austenitic stainless steel Workpiece surface continues the argon gas that through-current capacity is 7000 sccm, in the mobile machined electrode of austenite stainless steel workpiece surface, makes to discharge Processing speed is controlled in 1 cm2/ min, process time are 2 h, cut off the power supply of metal surface enhanced processor after processing is completed, It is further continued for logical argon gas 10min, austenite stainless steel workpiece is made to be cooled to room temperature.
Embodiment 2:
The concentration of sodium chloride solution is 15 wt. %, step to present embodiment in step (2) unlike the first embodiment (4) DC voltage is 90 V in, and other steps and parameter are same as Example 1.
Embodiment 1 and embodiment 2 are obtained that treated, and austenitic stainless steel carries out wear-resisting property test,
Under above-mentioned process conditions, high entropy alloy coating can be prepared in austenite stainless steel surface, and be remarkably improved Austria The wearability of family name's body stainless steel surface.As shown in Figure 1, the X-ray diffractogram and high-entropy alloy electrode material of high entropy alloy coating X-ray diffractogram it is consistent, it was demonstrated that high entropy alloy coating can be prepared using the present invention, Fig. 2 is shown, untreated austenite The wear weight loss of high entropy alloy coating and GCr15 opposite grinding that stainless steel and embodiment 1 obtain, Fig. 3 show that untreated austenite is not The high entropy alloy coating and Si that rust steel and embodiment 1 obtain3N4The wear weight loss of opposite grinding, Fig. 4 show untreated austenitic stainless steel With embodiment 2 obtain high entropy alloy coating and GCr15 opposite grinding wear weight loss, Fig. 5 show untreated austenitic stainless steel with The high entropy alloy coating and Si that embodiment 2 obtains3N4The wear weight loss of the wear weight loss of opposite grinding, untreated austenitic stainless steel is equal Much higher than high entropy alloy coating, illustrate that high entropy alloy coating has good wearability.Test data is shown in Table 1.In above-mentioned technique Under the conditions of, the high entropy alloy coating that austenite stainless steel surface obtains has good wearability.
Table 1
The wear test test result provided by table 1: the wear weight loss of high entropy alloy coating is far below untreated Austenitic stainless steel test piece.From the above results, surface preparation high entropy alloy coating after austenitic stainless steel obtain it is excellent Different wearability.

Claims (4)

1. a kind of preparation method of austenite stainless steel surface high entropy alloy coating, it is characterised in that: first to austenite stainless Steel carries out electrochemical etching processing, then prepares high entropy alloy coating again;The following steps are included:
(1) austenite stainless steel workpiece is pre-processed: silicon carbide waterproof abrasive paper will be used after austenitic stainless steel strip oil removing It is polished step by step, distilled water ultrasonic cleaning, drying for standby;
(2) the austenitic stainless steel test piece pre-processed is reserved into working face, rest part uses epoxy resin sealing, drying Afterwards, as working electrode, the sodium chloride solution that mass percent is the % of 10 % ~ 25 is placed in reference electrode and auxiliary electrode In, three-electrode system is formed, electrochemical etching processing is carried out to austenitic stainless steel test piece using electrochemical workstation, obtains Austria Family name's body stainless steel work-piece;
(3) the austenite stainless steel workpiece that step (2) is handled well is connect with the cathode of metal surface enhanced processor power supply, at For workpiece pole, then by fixture comb shape high-entropy alloy is connect with the anode of metal surface enhanced processor power supply, becomes and add Work electrode;
(4) power supply for connecting metal surface enhanced processor, adjust the DC voltage between workpiece pole and machined electrode be 80 V ~ 100 V, when the distance between workpiece pole and machined electrode are lower than 0.1 mm, the air between workpiece pole and machined electrode is electric From generation gas discharge phenomenon starts the preparation for carrying out high entropy alloy coating to austenite stainless steel workpiece;
(5) continue the argon gas that through-current capacity is 6000~8000 sccm to austenite stainless steel workpiece surface, in austenite stainless Steel workpiece surface moves machined electrode, makes electro-discharge machining rate control in 0.5~1.5 cm2/ min, process time are 1.5~3 H cuts off the power supply of metal surface enhanced processor after processing is completed, is further continued for logical 5~15 min of argon gas, makes austenitic stainless steel Workpiece is cooled to room temperature, and high entropy alloy coating is made;
The austenitic stainless steel is 316L austenitic stainless steel;The high-entropy alloy is AlCrCuFeNi2The high entropy of multicomponent closes Gold.
2. the preparation method of austenite stainless steel surface high entropy alloy coating according to claim 1, it is characterised in that: institute The mass percent for stating sodium chloride solution is 15 % or 20 %.
3. the preparation method of austenite stainless steel surface high entropy alloy coating according to claim 1, it is characterised in that: institute Stating reference electrode is saturated calomel electrode;The auxiliary electrode is platinized platinum.
4. the preparation method of austenite stainless steel surface high entropy alloy coating according to claim 1, it is characterised in that: step Suddenly in (5), the DC voltage is 80 V or 90 V, and processing speed is 1 cm2/ min, process time are 2 h.
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CN106756236A (en) * 2016-12-31 2017-05-31 镇江市丹徒区硕源材料科技有限公司 A kind of TC19 titanium alloy composite materials and its preparation method and application
CN108728876B (en) * 2018-06-06 2020-08-07 西南石油大学 Preparation method of FeCoNiCuMo high-entropy alloy film
CN112501569B (en) * 2020-12-18 2022-08-16 哈尔滨工业大学(深圳) Surface gradient high-entropy alloy layer and preparation method thereof

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